气相色谱-质谱联用技术测定饮用水中的二氯乙酸和三氯乙酸  

Determination of dichloroacetic acid and trichloroacetic acid in drinking water by gas chromatography-mass spectrometry

作　　者：郑建峰 郑亚萍 ZHENG Jian-Feng;ZHENG Ya-Ping(Zhejiang Pharmaceutical Co.,Ltd.,Changhai Biological Branch,Shaoxing 312000,China;Zhejiang Changhai Pharmaceutical Co.,Ltd.,Shaoxing 312000,China)

机构地区：[1]浙江医药股份有限公司昌海生物分公司,绍兴312000 [2]浙江昌海制药有限公司,绍兴312000

出　　处：《实验室检测》2024年第8期4-7,共4页Laboratory Testing

摘　　要：目的 建立一种快速、准确、灵敏的气相色谱-质谱联用(GC-MS)方法,用于检测饮用水样品中的二氯乙酸(DCA)和三氯乙酸(TCA),并评估该方法的性能和实际应用效果。方法 采用液-液萃取衍生化技术对样品进行前处理,然后利用GC-MS进行分析。分别以50μL和100μL的DCA和TCA标准品配制成浓度分别为5μg/mL和10μg/mL的母液,再用甲醇梯度稀释成一系列浓度梯度的标准溶液,用于建立标准曲线。以1,2-二溴丙烷为内标物质,配制成166.1μg/L的内标萃取液,用于校正样品分析过程中的误差。对超纯水进行加标回收实验,评估方法的准确性和精密度,利用信噪比(S/N)法确定方法的检出限。最后,对103份生活饮用水样品进行检测,分析DCA和TCA的含量。结果 标准曲线线性范围分别为DCA 1~20μg/mL和TCA 1~40μg/mL,相关系数(r^(2))均大于0.99,回收率为99.4%~114.3%,RSD小于3.541%,DCA和TCA的检出限分别为0.1μg/L和0.2μg/L。103份生活饮用水样品中DCA和TCA的含量均低于国家标准限值,平均浓度分别为0.25μg/L和0.48μg/L,数据具有统计学意义(P<0.05)。结论 该GC-MS方法具有良好的线性、准确性、精密度和灵敏度,能够满足饮用水安全监测的需求。应用该方法对103份生活饮用水样品进行检测,结果表明饮用水水质符合国家标准,未受到DCA和TCA的严重污染。Objective To establish a rapid,accurate and sensitive gas chromatography-mass spectrometry(GC-MS)method for the detection of dichloroacetic acid(DCA)and trichloroacetic acid(TCA)in drinking water samples,and to evaluate the performance and practical application of the method.Methods The samples were pretreated by liquid-liquid extraction derivatization technology and then analyzed by GC-MS.50μL and 100μL of DCA and TCA standards were prepared into mother solutions with concentrations of 5μg/mL and 10μg/mL,respectively,and then diluted with methanol to form a series of standard solutions with concentration gradients for the establishment of standard curves.1,2-Dibromopropane was used as the internal standard substance to prepare an internal standard extract of 166.1μg/L to correct the error in the sample analysis process.The spike recovery experiment was carried out on ultrapure water to evaluate the accuracy and precision of the method,and the detection limit of the method was determined by the signal-to-noise ratio(S/N)method.Finally,103 drinking water samples were tested to analyze the contents of DCA and TCA.Results The linear ranges of the standard curves were 1~20μg/mL for DCA and 1~40μg/mL for TCA,with correlation coefficients(r^(2))greater than 0.99,recoveries of 99.4%~114.3%,RSDs less than 3.541%,and detection limits of 0.1μg/L and 0.2μg/L for DCA and TCA,respectively.The contents of DCA and TCA in 103 drinking water samples were lower than the national standard limits,with average concentrations of 0.25μg/L and 0.48μg/L,respectively,and the data were statistically significant(P<0.05).Conclusion The GC-MS method has good linearity,accuracy,precision and sensitivity,and can meet the needs of drinking water safety monitoring.The method was applied to 103 drinking water samples,and the results showed that the drinking water quality met the national standards and was not seriously contaminated by DCA and TCA.

关 键 词：气相色谱 饮用水 二氯乙酸 三氯乙酸 水质检测 

分 类 号：O657.63[理学—分析化学] R123.1[理学—化学]